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Triethylamine → HCID 24860699, 화합물

HRID 1258461
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HRID 1258461 반응식
[CH3:1][O:2][CH2:3][CH2:4][N:5]1[C:9]2[C:10]3[O:11][CH:12]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[CH2:13][CH2:14][C:15]=3[C:16]([C:18](O)=[O:19])=[CH:17][C:8]=2[N:7]=[C:6]1[CH3:27].[CH2:28]([N:30](CC)[CH2:31]C)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.Cl.CNC>CN(C)C=O>[CH3:1][O:2][CH2:3][CH2:4][N:5]1[C:9]2[C:10]3[O:11][CH:12]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[CH2:13][CH2:14][C:15]=3[C:16]([C:18]([N:30]([CH3:31])[CH3:28])=[O:19])=[CH:17][C:8]=2[N:7]=[C:6]1[CH3:27]
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반응물 4

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67220219HCID 67220219, 화합물

생성물 1

HCID 24860699HCID 24860699, 화합물

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of 1-(2-methoxyethyl)-2-methyl-8-phenyl-1,6,7,8-tetrahydrochromeno[7,8-d]imidazole-5-carboxylic acid (200 mg, 0.55 mmol, Step 12), triethylamine (0.30 mL, 2.18 mmol), and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium hexafluorophosphate (228 mg, 0.60 mmol) in N,N-dimethylformamide (5 mL) was added dimethylamine hydrochloride (49 mg, 0.60 mmol) at 0° C. After stirring at room temperature for 12 h, the mixture was poured onto water, and the aqueous layer was extracted with dichloromethane. The combined organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with dichloromethane/methanol (20:1) to afford the title compound as a white amorphous (215 mg, quant.).

후처리

  1. additionthe mixture was poured onto water
  2. extractionthe aqueous layer was extracted with dichloromethane
  3. dry with materialThe combined organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane/methanol (20:1)

출처 및 근거

ORD 기록
ord-95867aac19084ab5945ca30112d5a53f
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08466166B2

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